ChemicalBook CAS DataBase List 3,5-DINITROANISOLE

3,5-DINITROANISOLE synthesis

9synthesis methods

Product Name:3,5-DINITROANISOLE
CAS Number:5327-44-6
Molecular formula:C7H6N2O5
Molecular Weight:198.13

124-41-4 Synthesis

124-41-4
685 suppliers
$12.00/25g

97-00-7
12 suppliers
$17.67/10gm:

5327-44-6
39 suppliers
$75.00/2g

Yield:5327-44-6 99.4%

Reaction Conditions:

in methanol at 50 - 60;Large scale;

Steps:

1-3 Preparation 2,4-dinitroanisole Example 3:

Add 300 kg of methanol to the 2000L reactor and start stirring; add 150 kg of 2,4-dinitrochlorobenzene, and when the temperature rises to 50-55 °C, start adding sodium methoxide (sodium methoxide) purchased at a uniform rate the content is 29% solution, the amount of addition is 2,4-dinitrochlorobenzene: sodium methoxide = 1: (1 ~ 1.01) (molar ratio), the temperature of the reaction kettle should not exceed 60 °C when feeding, the feeding time is controlled within 50-60min. After adding sodium methoxide, keep the temperature at this temperature for 15min, add 300 kg of washing water at this temperature, recover methanol under vacuum, add an appropriate amount of hydrochloric acid, adjust the pH value of the system to be neutral, after the operation is completed, the material filter and wash with 150 kg of water. The solid material after filtration is dried to obtain 149.1 kg of 2,4-dinitroanisole, melting point: 95.6°C, purity: 99.6% (chromatographic analysis), 2,4-dinitrobenzene fraction: 0.02%, yield: 99.4%.

References:

CN111187168,2020,A Location in patent:Paragraph 0049-0054